Applications of scanning optical microscopy in materials science to detect bulk microdefects in semiconductors

A three-dimensional atom probe permits the elemental reconstruction of a small volume of a specimen by determining the x , y and z positions and mass-to-charge ratio of the atoms in that volume. The historical development of this new type of atom probe is described. Several variants of these instruments including the position-sensitive atom probe, the optical atom probe and the tomographic atom probe are reviewed. The various methods of data visualization and analysis are summarized. The performance of the three-dimensional atom probe is compared with the energy-compensated atom probe.     

Some aspects of the field evaporation behaviour of GaSb

In-depth analysis of pulsed laser atom probe tomography (APT) data on the field evaporation of the III-V semiconductor material GaSb reveals strong variations in charge states, relative abundances of different cluster ions, multiplicity of detector events and spatial correlation of evaporation events, as a function of the effective electric field at the specimen surface. These variations are discussed in comparison with the behaviour of two different metallic specimen materials, an Al-6XXX series alloy and pure W, studied under closely related experimental conditions in the same atom probe instrument. It is proposed that the complex behaviour of GaSb originates from a combination of spatially correlated evaporation events and the subsequent field induced dissociation of cluster ions, the latter contributing to inaccuracies in the overall atom probe composition determination for this material.     

Characterisation of the early stages of solute clustering in 1Ni–1.3Mn welds containing Cu

Microstructural characterisation of neutron irradiated low alloy steels is important for developing mechanistic understanding of irradiation embrittlement. This work is focused on the early stages of irradiation-induced clustering in a low Cu (0.03 wt%), high Ni (∼1 wt%) weld. The weld was irradiated at a very high dose rate and then examined by atom probe (energy-compensated position-sensitive atom probe (ECOPoSAP) and local electrode atom probe (LEAP)) with supporting microstructural information obtained by small angle neutron scattering (SANS) and positron annihilation (PALA).     

Fabrication of specimens of metamorphic magnetite crystals for field ion microscopy and atom probe microanalysis.

Field ion specimens have been successfully fabricated from samples of metamorphic magnetite crystals (Fe3O4) extracted from a polymetamorphosed, granulite-facies marble with the use of a focused ion beam. These magnetite crystals contain nanometer-scale, disk-shaped inclusions making this magnetite particularly attractive for investigating the capabilities of atom probe field ion microscopy (APFIM) for geological materials. Field ion microscope images of these magnetite crystals were obtained in which the observed size and morphology of the precipitates agree with previous results. Samples were analyzed in the energy compensated optical position-sensitive atom probe. Mass spectra were obtained in which peaks for singly ionized 16O, 56Fe and 56FeO and doubly ionized 54Fe, 56Fe and 57Fe peaks were fully resolved. Manganese and aluminum were observed in a limited analysis of a precipitate in an energy compensated position sensitive atom probe.     

Characterization of dilute species within CVD‐grown silicon nanowires doped using trimethylboron: protected lift‐out specimen preparation for atom probe tomography

Three‐dimensional quantitative compositional analysis of nanowires is a challenge for standard techniques such as secondary ion mass spectrometry because of specimen size and geometry considerations; however, it is precisely the size and geometry of nanowires that makes them attractive candidates for analysis via atom probe tomography. The resulting boron composition of various trimethylboron vapour–liquid–solid grown silicon nanowires were measured both with time‐of‐flight secondary ion mass spectrometry and pulsed‐laser atom probe tomography. Both characterization techniques yielded similar results for relative composition. Specialized specimen preparation for pulsed‐laser atom probe tomography was utilized and is described in detail whereby individual silicon nanowires are first protected, then lifted out, trimmed, and finally wet etched to remove the protective layer for subsequent three‐dimensional analysis.     

Standard deviations of composition measurements in atom probe analyses. Part I conventional 1D atom probe

Atom probe is a very powerful instrument to measure concentrations on a sub nanometric scale [M.K. Miller, G.D.W. Smith, Atom Probe Microanalysis, Principles and Applications to Materials Problems, Materials Research Society, Pittsburgh, 1989]. Atom probe is therefore a unique tool to study and characterise finely decomposed metallic materials. Composition profiles or 3D mapping can be realised by gathering elemental composition measurements. As the detector efficiency is generally not equal to 1, the measured compositions are only estimates of actual values. The variance of the estimates depends on which information is to be estimated. It can be calculated when the detection process is known. These two papers are devoted to give complete analytical derivation and expressions of the variance on composition measurements in several situations encountered when using atom probe. In the first paper, we will concentrate on the analytical derivation of the variance when estimation of compositions obtained from a conventional one dimension (1D) atom probe is considered. In particular, the existing expressions, and the basic hypotheses on which they rely, will be reconsidered, and complete analytical demonstrations established. In the second companion paper, the case of 3D atom probe will be treated, highlighting how the knowledge of the 3D position of detected ions modifies the analytical derivation of the variance of local composition data.     

Determining the composition of small features in atom probe: bcc Cu-rich precipitates in an Fe-rich matrix

Aberrations in the ion trajectories near the specimen surface are an important factor in the spatial resolution of the atom probe technique. Near the boundary between two phases with dissimilar evaporation fields, ion trajectory overlaps may occur, leading to a biased measurement of composition in the vicinity of this interface. In the case of very small second-phase precipitates, the region affected by trajectory overlaps may extend to the centre of the precipitate prohibiting a direct measurement of composition. A method of quantifying the aberrant matrix contribution and thus estimating the underlying composition is presented. This method is applied to the Fe–Cu-alloy system, where the precipitation of low-nanometre size Cu-rich precipitates is of considerable technical importance in a number of materials applications. It is shown definitively that there is a non-zero underlying level of Fe within precipitates formed upon thermal ageing, which is augmented and masked by trajectory overlaps. The concentration of Fe in the precipitate phase is shown to be a function of ageing temperature. An estimate of the underlying Fe level is made, which is at lower levels than commonly reported by atom probe investigations.     

Atom probe trajectory mapping using experimental tip shape measurements

Atom probe tomography is an accurate analytical and imaging technique which can reconstruct the complex structure and composition of a specimen in three dimensions. Despite providing locally high spatial resolution, atom probe tomography suffers from global distortions due to a complex projection function between the specimen and detector which is different for each experiment and can change during a single run. To aid characterization of this projection function, this work demonstrates a method for the reverse projection of ions from an arbitrary projection surface in 3D space back to an atom probe tomography specimen surface. Experimental data from transmission electron microscopy tilt tomography are combined with point cloud surface reconstruction algorithms and finite element modelling to generate a mapping back to the original tip surface in a physically and experimentally motivated manner. As a case study, aluminium tips are imaged using transmission electron microscopy before and after atom probe tomography, and the specimen profiles used as input in surface reconstruction methods. This reconstruction method is a general procedure that can be used to generate mappings between a selected surface and a known tip shape using numerical solutions to the electrostatic equation, with quantitative solutions to the projection problem readily achievable in tens of minutes on a contemporary workstation.     

An optical non-contact probe

An optical non-contact probe to detect displacement, position and inclination of a work surface is presented. It uses two light beams which intersect near the surface and form spots of light on it. Images of the spots are formed on a photo-detector by a lens. Positions of the images and distance between them, which depend on the distance from the intersection to the surface, are sensed by the detector. Its output is electrically converted into a signal which represents displacement, position or inclination of the surface. An experimental probe is set up, in which laser diodes and a position-sensitive detector are used. The probe is tested on sandy, milled, lathe-turned, ground and specular surfaces and the measurements agree with predicted values.     

Impact of laser pulsing on the reconstruction in an atom probe tomography

The implementation of fast pulsed laser has significantly improved the performance of the atom probe technique by enabling near-atomic-scale three-dimensional analysis of poorly conducting materials. This has broadened the range of applications for the atom probe, addressing a major limitation of the technique. Despite this, the implications of lasing on the tomographic reconstruction of atom probe data have yet to be fully characterised. Here, we demonstrate how changes in the shape of the specimen surface, induced by laser pulsing, affect the ion trajectories, and hence the projection parameters used to build the three-dimensional map.     

Analysis conditions of an industrial Al-Mg-Si alloy by conventional and 3D atom probes.

Industrial 6016 Al-Mg-Si(Cu) alloys are presently regarded as attractive candidates for heat treatable sheet materials. Their mechanical properties can be adjusted for a given application by age hardening of the alloys. The resulting microstructural evolution takes place at the nanometer scale, making the atom probe a well suited instrument to study it. Accuracy of atom probe analysis of these aluminium alloys is a key point for the understanding of the fine scale microstructural evolution. It is known to be strongly dependent on the analysis conditions (such as specimen temperature and pulse fraction) which have been widely studied for ID atom probes. The development of the 3D instruments, as well as the increase of the evaporation pulse repetition rate have led to different analysis conditions, in particular evaporation and detection rates. The influence of various experimental parameters on the accuracy of atom probe data, in particular with regard to hydride formation sensitivity, has been reinvestigated. It is shown that hydrogen contamination is strongly dependent on the electric field at the specimen surface, and that high evaporation rates are beneficial. Conversely, detection rate must be limited to smaller than 0.02 atoms/pulse in order to prevent drastic pile-up effect.     

A novel atomic force microscope operating in liquid for in situ investigation of electrochemical preparation of porous alumina

A novel atomic force microscope (AFM) operating in liquid is described in this article. The specially designed AFM probe involves a tip attached to a cantilever, a tip holder, and a circular Plexiglas window. When the probe dives into the fluid, a circular meniscus is established around the Plexiglas window, preventing the tip from being affected or destroyed by surface tension of the liquid. In this setup, the whole scanning probe and the sample can completely dive into fluid. Meanwhile, the probe tip scans over the sample surface when the instrument works. These advantages enable the instrument to scan comparatively large or heavy samples with a high speed. The highest scan rate is about 30 lines/s or 14 s for a 400 x 400-pixel, 3 x 3 microm image. Using the new AFM, we carry out in-situ investigation of the formation processes of porous alumina during electrochemical anodic oxidation. A lead ring and an aluminum foil serve as cathode and anode, respectively. They are entirely immersed in the bath electrolyte, which is oxalic acid solution. During anodic oxidation, the AFM images of the sample surface are successively acquired without elevating the sample out of the solution. Experiments reveal that electrochemical reactions take place soon after the power supply is switched on, and with the progression of anodization, nanostructures of porous alumina gradually occur on the aluminum substrate, finally yielding ordered arrays of nanopores. As a typical example of applications, the results of this work show that the new AFM is an ideal and powerful tool for in-situ observation and study of materials or samples in aqueous solutions.     

New tomographic atom probe at University of Muenster, Germany

Currently atom probe tomography provides the highest spatial resolution compared to all other volume analysis techniques. Owing to its single atom sensitivity, it is specially suited to study nano-structured materials. Therefore, a new atom probe was installed at the Institute for Material Physics at University of Muenster, Germany, to study thin film reactions. Since the available budget was rather limited, a cost-effective non-commercial atom probe was constructed. The instrument is based on a 2D delay line detector system of 120 mm diameter. To achieve a large collecting angle and thus large volumes of analysis, a straight flight tube without a reflectron is used. This way, the flight distance may be reduced down to 160 mm. However, the variable chamber layout allows using a reflectron as an alternative. Furthermore, a laser system is implemented that delivers pulses in the 500 ps range to make possible laser-assisted evaporation of atoms. The article describes instrumental details and presents first characteristic data.     

Hybrid integrated sensor for position measurement

The design, fabrication and performance of an integrated two-dimensional position-sensitive photodetector are presented. The optoelectronic device used as the sensitive element in the circuit is a full-area position-sensitive photodiode (PPD) with high linearity over the full sensitive area. The PPD is integrated with the analogue electronics in a hybrid circuit using thick film technology. The analogue electronics include the signal amplification and the signal conditioning to form the output signals proportional to the light beam centre position at the sensor surface and an output signal proportional to the light beam intensity. Using hybrid integration, a new position-sensitive transducer is developed, giving output signals which can transmit above large distances without problems and drive directly actuators in any control system.     

Atom probe,AFM, and STM studies on vacuum-fired stainless steels

The surface morphology of grades 304L and 316LN stainless steels, after low-temperature bake-out process and vacuum annealing, has been studied by atomic force microscopy (AFM) and scanning tunnelling microscopy (STM). The local elemental composition on the surface before and after thermal treatment has been investigated by atom probe (AP) depth profiling measurements. After vacuum annealing, AFM and STM show significant changes in the surface structure and topology. Recrystallization and surface reconstruction is less pronounced on the 316LN stainless steel. AP depth profiling analyses result in noticeable nickel enrichment on the surface of grade 304L samples. Since hydrogen recombination is almost controlled by surface structure and composition, a strong influence on the outgassing behaviour by the particular surface microstructure can be deduced.     

Optimal design and fabrication of three-dimensional calibration specimens for scanning probe microscopy

Micro-/nano-scale roughness specimens are highly demanded to synthetically calibrate the scanning probe microscopy (SPM) instrument. In this study, three-dimensional (3D) specimens with controllable main surface evaluation parameters were designed. In order to improve the design accuracy, the genetic algorithm was introduced into the conventional digital filter method. A primary 3D calibration specimen with the dimension of 10 μm × 10 μm was fabricated by electron beam lithography. Atomic force microscopy characterizations demonstrated that the statistical and spectral parameters of the fabricated specimen match well with the designed values. Such a kind of 3D specimens has the potential to calibrate the SPM for applications in quantitative surface evaluations.     

Heterodyning based portable instrument for eddy currents non-destructive testing

The development and implementation of a portable eddy currents testing instrument with heterodyning based measurements is presented in this paper. The instrument is composed by a dedicated electronic measurement circuitry embedded inside a rugged tablet computer for control and visualization and that interfaces a small footprint planar eddy currents probe. A DDS waveform generator and a transconductance amplifier are used to drive the probe current. The probe output voltage is amplified up to 60 dB and down-converted to an intermediary frequency, which is then digitized. IQ demodulation of the digitized signal is used to obtain the real and imaginary components of the probe output and is computed in real time by the embedded digital signal processor and transmitted to the host computer by USB. The eddy currents testing instrument can be operated as a battery powered standalone device with post-processing and visualization capabilities which can be modified for specific applications without the need for hardware modifications. The system architecture, electrical characterization of the analog circuit, digital signal processing and visualization interface are described. The eddy currents inspection results of an aluminum sample with synthetic defects and friction stir welding joint samples, using this instrument are presented.     

Using Kelvin probe force microscopy for controlling the phase composition of austenite–martensite chromium–nickel steel

The effectiveness of Kelvin probe force microscopy, which is one of the scanning probe techniques, is demonstrated for assessing plastic-deformation induced changes in the phase composition of 08Kh21N6M2T austenite–martensite chromium–nickel steel. Changes in the numerical values of surface potentials of different phase components of two- and three-phase stainless steels versus sample deformation extent have been established. Dependence of surface electric potentials as measured with Kelvin probe force microscopy on the presence and amount of newly formed deformationmartensite phase has been discovered.     

离子质谱计及其应用

文章介绍了离子质谱计的原理及应用范围。由快原子枪装备的一台低价小型双聚焦质谱计用于离子的同位素丰度分析,微克级氮的同位素测量精度为1.5％。列举了一些应用实例,如用~(15)N、~(10)B和~(42)Ca、~(44)Ca作示踪剂研究生物学过程。     

Identification of phases in gas-atomised droplets by combination of neutron and X-ray diffraction techniques with atom probe tomography

Powders of Al_68.5Ni_31.5 alloy have been produced by gas atomisation and sieved in different grain size families. The resulting families have been analysed by combined neutron and X-ray diffraction in order to investigate the structure and identify the existing phases at the surface and in the bulk of the grains. The weight fraction of the identified phases (Al₃Ni₂, Al₃Ni and Al) has been estimated from a profile refinement with the FULLPROF computer codes. An additional phase was observed but could not be identified in the diffraction patterns. Starting from grains less than 5 μm in diameter, samples have been shaped by annular focused ion beam into needles that were suitable for atom probe investigations. The structure and morphologies observed by different techniques are compared and discussed. It has also been possible to estimate the crystallite sizes and the strains corresponding to the different phases present in the powders from the refinement of the ND patterns. In addition to Al₃Ni₂ and Al₃Ni, a phase of composition close to the nominal one of the alloy was observed in the atom probe measurements. This phase could be one of the decagonal ones referred to in the literature. Small particles of composition close to Al₈₂Ni₁₈ are attributed to the metastable Al₉Ni₂ phase. The achieved conclusions demonstrate the complementarity of X-ray and neutron diffraction techniques and atom probe tomography to analyse complex structures.